US9259785B2 - Method for the densification and spheroidization of solid and solution precursor droplets of materials using microwave generated plasma processing - Google Patents
Method for the densification and spheroidization of solid and solution precursor droplets of materials using microwave generated plasma processing Download PDFInfo
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- US9259785B2 US9259785B2 US14/700,847 US201514700847A US9259785B2 US 9259785 B2 US9259785 B2 US 9259785B2 US 201514700847 A US201514700847 A US 201514700847A US 9259785 B2 US9259785 B2 US 9259785B2
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/026—Spray drying of solutions or suspensions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B9/00—Making granules
- B29B9/16—Auxiliary treatment of granules
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/62645—Thermal treatment of powders or mixtures thereof other than sintering
- C04B35/62655—Drying, e.g. freeze-drying, spray-drying, microwave or supercritical drying
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05H—PLASMA TECHNIQUE; PRODUCTION OF ACCELERATED ELECTRICALLY-CHARGED PARTICLES OR OF NEUTRONS; PRODUCTION OR ACCELERATION OF NEUTRAL MOLECULAR OR ATOMIC BEAMS
- H05H1/00—Generating plasma; Handling plasma
- H05H1/24—Generating plasma
- H05H1/26—Plasma torches
- H05H1/30—Plasma torches using applied electromagnetic fields, e.g. high frequency or microwave energy
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
- B22F2009/0836—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid with electric or magnetic field or induction
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
- B22F2009/086—Cooling after atomisation
- B22F2009/0872—Cooling after atomisation by water
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B9/00—Making granules
- B29B9/10—Making granules by moulding the material, i.e. treating it in the molten state
Definitions
- the present invention is generally directed to a method for taking feed material and processing the feed material to produce dense and spheroidal products.
- the feed material is comprised of powder particles from the spray-drying technique or solution precursor droplets containing ceramic or metallic materials. More particularly, the present invention is directed to a method which uses a microwave plasma torch capable of generating a laminar flow pattern during materials processing to produce dense and spheroidal products.
- the laminar flow in an axisymmetric hot zone with a uniform temperature profile within the torch allows for the production of uniform spheroidal particles with a homogenous materials distribution, which leads to final products possessing superior characteristics.
- Spheroidization process transforms powders produced by spray drying and sintering techniques, or angular powders produced by conventional crushing methods, into spheres.
- Spheroidized particles are more homogenous in shape, denser, much less porous, provide higher flowability, and possess lower friability. These characteristics make for powders that are superior for applications such as injection molding, thermal spraying of coatings and provide parts having near net shapes.
- thermal arc plasma an electric arc is produced between two electrodes and is then blown out of the plasma channel using plasma gas. Powder is then injected from the side, perpendicular or at an angle, into the plasma plume, where it gets exposed to the high temperature of the plasma and is collected as spheres in filters during subsequent processing.
- An issue with thermal arc plasma is that the high temperature of the electrodes leads to erosion of the electrodes, which leads to contamination of the plasma plume with the electrode material, resulting in the contamination of the powders to be processed.
- the thermal arc plasma plume has an inherently uneven temperature gradient, and by injecting powder into the plasma plume from the side, the powder gets exposed to an uneven temperature gradient that leads to the production of particles that are not homogenous in size, density or porosity.
- Radio frequency plasmaspheroidization the plasma is produced in a dielectric cylinder by induction at atmospheric pressure.
- Radio frequency plasmas are known to have low coupling efficiency of the radio frequency energy into the plasma and a lower plasma temperature compared to arc and microwave generated plasmas.
- the magnetic field responsible for generating the plasma in radio-frequency plasma is non-uniform in profile which leads to an uneven temperature gradient and thus a non-homogenous thermal treatment of the particles. This leads to non-homogeneity in size, microstructure, and density or porosity of the final product.
- a pressurized powder feeder is used to axially inject powder particles into a plasma chamber where the powder particles are entrained in a laminar gas flow pattern and undergo uniform heat treatment by being exposed to a uniform temperature profile within the microwave generated plasma. This results in spheroidal pearl-like particles having uniform density.
- a droplet maker or atomizer is used to inject solution precursor droplets which are entrained in a laminar gas flow pattern and undergo uniform heat treatment by being exposed to a uniform temperature profile within the microwave generated plasma to produce spheroidal pearl-like particles having uniform density.
- Another feature of this invention is that it uses microwave generated plasma in accordance with U.S. patent application Ser. No. 13/445,947.
- an object of the present invention is to provide a laminar flow environment, free of turbulent flow effects, for the feed material that is processed with the microwave generated plasma, which results in dense and spheroidal particles having uniform sizes and shapes and characterized by a homogenous materials distribution.
- FIG. 2A illustrates densified and spheroidized MgO—Y 2 O 3 particles obtained by the microwave plasma process after injection of spray-dried powder
- FIG. 2B illustrates the size of the densified and spheroidized MgO—Y 2 O 3 particles obtained by the microwave plasma process after injection of spray-dried powder by reference to the scales on a ruler;
- FIG. 2 illustrates densified and spheroidized MgO—Y 2 O 3 particles obtained by the microwave plasma process after injection of spray-dried powder
- FIG. 3 illustrates a method of atomizing droplets using a nebulizing apparatus
- FIG. 4 illustrates densified and spheroidized 7% by weight Y 2 O 3 —ZrO 2 (7YSZ) ceramic particles, 20 to 38 micrometers in diameter after injection of 7YSZ precursor droplets using a nebulizing injector;
- FIG. 5 illustrates densified and spheroidized 7YSZ ceramic particles, 38 to 53 micrometers in diameter after injection of 7YSZ precursor droplets using a nebulizing injector;
- FIG. 6 illustrates a method of spheroidization by injection of solid powder using a powder feeder
- FIG. 7 illustrates a method of spheroidization by injection of a mist of droplets using a nebulizing nozzle
- FIG. 8 illustrates a method of spheroidization by injection of a continuous stream of uniform droplets using a frequency driven droplet maker.
- an apparatus to produce dense and spheroidal products which includes a microwave radiation generator 1 , a plasma chamber 2 , a dielectric sheathing plasma torch 3 , and a powder feeder, or solution precursor injector, 4 .
- the microwave radiation generator 1 described in US Patent Publication 2008/0173641 A1 is combined with plasma chamber 2 and plasma sheathing torch 3 . Both 2 and 3 are described in U.S. patent application Ser. No. 13/445,947.
- the particle feeder 4 is an injection apparatus with a pressurized source 5 that can feed solid powder particles 6 into dielectric plasma torch 3 . When powder injection is used, particles 6 may be a product of spray-drying techniques or other techniques.
- particles 6 may be droplets of solution precursor injected using an atomizer, or a droplet maker energized with a high frequency electrical drive.
- Pressurized sources 7 and 8 are used to introduce process gases as inputs into 3 to entrain and accelerate particles 6 along axis 11 towards plasma 14 .
- particles 6 are accelerated by entrainment using core laminar gas flow 10 created through annular gap 9 .
- Cooling laminar flow 13 created through annular gap 12 flows at not lower than 100 standard cubic feet per hour in the case of solid powder feed or atomized injection, and provides laminar sheathing for the inside wall of dielectric torch 3 to protect it from melting due to heat radiation from plasma 14 .
- High flow is also needed to keep particles 6 from reaching the inner wall of 3 where plasma attachment could take place.
- Relatively lower gas flows are needed when using a droplet maker injector as the flow of particles is more uniform and follows axis 11 closely.
- Particles 6 are guided by laminar flows 10 and 13 towards microwave plasma 14 were they undergo homogeneous thermal treatment to become dense and spherical product particles 15 .
- the densification and spheroidization of spray-dried ceramic solid particles 6 , or of droplets of solution precursor materials, is achieved by choosing the appropriate experimental parameters capable of maintaining a stable microwave generated plasma 14 to produce dense and spherical particles 15 .
- microwave power in 1 powder particles or solution precursor droplet injection flow rates along axis 11 , carrier gas flow rates of laminar entrainment flow 10 , laminar cooling flow 13 inside the dielectric sheathing torch 3 , heating rates within plasma 15 and quenching rates not less than 10 30 C/sec upon exit of plasma 15 .
- this method has been applied to spheroidize particles 6 made of commercial Magnesia-Yttria (MgO—Y 2 O 3 ) solid powder particles obtained by the spray-drying technique of the INFRAMAT Corporation.
- Particles 6 in the case of INFRAMAT powder, possess closed or semi-spherical morphology, low density, and are highly porous and brittle particles.
- the powder feeder 4 with a reservoir with low pressure gas flow ( ⁇ 20 PSI) from pressurized source 5 , provides a fluidized bed for particles 6 which are driven by gas flow through powder feeder 4 towards the input of plasma torch 3 .
- Particles 6 diameters initially ranged between 38 micrometers ( ⁇ m) and 73 ⁇ m.
- the elimination of small particles prior to injection reduces any recirculation of materials above the hot zone.
- the elimination of large particles reduces the diameter range of particle products that will be collected.
- Sieves with mesh size 400 (38 ⁇ m), and 200 (74 ⁇ m) have been used to accomplish this classification.
- Particles 6 are then entrained and accelerated along axis 11 by laminar gas flow 10 for a minimum distance of two (2) inches towards microwave plasma 14 .
- Laminar flow 10 is crucial in constraining the flow paths of particles 6 to a cylindrical region as close as possible to axis 11 .
- the penetration into plasma 14 is accomplished in such a manner that directional paths of particles 6 take place at the center of plasma 14 along axis 11 .
- Particles 6 are again accelerated, in part, by a second laminar gas flow 13 , over a minimum distance of three quarters of an inch before reaching the top of the plasma flame 14 .
- the primary function of laminar flow 13 is to ensure adequate cooling of the dielectric tube sheath 3 that houses the plasma.
- Laminar flow 13 need to be high enough to span the remainder of the length of the outer tube of dielectric plasma torch 3 .
- Two large ticks of the ruler in FIG. 2B correspond to 100 micrometers which demonstrates that particles 15 range in diameter from 15 micrometers to 50 micrometers.
- the densified and spheroidized particles 6 exhibit a “pearl” like texture and morphology.
- Nebulizer 16 consists of two concentric quartz tubes 17 and 18 which are fused together.
- a solution precursor of 7YSZ, or any other weight concentration of Yttrium ranging from 3% to 20%, in a pressurized stainless steel tank is introduced at input 19 of tube 17 .
- the solution precursor injection flow rate is in the order of 4 milliliters per minute and the gas tank pressure is about 20 pounds per square inch (PSI).
- PSI pounds per square inch
- the length of tube 18 is no smaller than 2 inches and does not exceed one foot.
- a pressurized gas source 21 pushes the atomizing gas flow 22 through an annular gap between concentric tubes 18 and 17 in nebulizer 16 .
- the injected solution precursor exits through orifice 23 where it is atomized by gas flow 22 , and exits at orifice 24 of tube 18 as an aerosol of droplet particles 6 .
- the distance between orifice 23 and orifice 24 must not exceed 1 millimeter (mm).
- the end of tube 18 is tapered so that gas flow 22 enters the jet of solution precursor with an angle close to 90 degrees.
- particles 6 are entrained by laminar flow 10 in dielectric plasma torch 3 , also seen in FIG. 1 , and subsequently the particles reach the axis-symmetric thermal processing medium inside dielectric plasma torch 3 where they undergo volumetric heating in plasma 14 .
- FIG. 4 and FIG. 5 these illustrate densified and spheroidized 7YSZ product particles 15 by atomizing 7YSZ solution precursor using nebulizer 16 .
- Particles 15 exhibit a “pearl” like texture and morphology. Particles 15 measure approximately between 20 micrometers ( ⁇ m) and 53 micrometers ( ⁇ m) in diameter as shown in FIG. 4 (20 to 38 ⁇ m), and FIG. 5 (38 to 53 ⁇ m) after post-classification with sieves having mesh sizes of 635 (20 ⁇ m), 400 (38 ⁇ m), and 270 (53 ⁇ m), respectively.
- the densified and spheroidized particles are made according to the procedure described therein.
- the powder particles to be processed are first sifted and classified according to their diameters, the minimum diameter is 20 ⁇ m and the maximum diameter is 74 ⁇ m. This eliminates recirculation of light particles above the hot zone of the plasma chamber and also ensures that the process energy present in the plasma is sufficient to melt the particles.
- This powder is then disposed in a powder feeder where a fluidized bed, in an internal chamber using a relatively low pressurized source of air not exceeding 20 pounds per square per inch (PSI), is introduced.
- PSI pounds per square per inch
- the powder feeder is constantly shaken using a shaker energized by another pressurized source of air having a minimum pressure of 20 pounds per square per inch (PSI).
- PSD pounds per square per inch
- the powder is carried from inside the powder feeder towards the input of the feeding tube of the dielectric plasma torch under pressure which permits a constant injection of particles into the plasma process.
- microwave radiation is introduced into the waveguide towards the plasma chamber where the dielectric plasma torch is located, and placed perpendicularly to the waveguide.
- Two annular flows are introduced; one for entrainment of injected particles and the other flow protects the inner wall of the outer tube of the plasma torch from melting under the effect of the high heat from the plasma.
- entrainment and cooling flows are chosen to stabilize the plasma.
- these entrainment and cooling flows are chosen to allow smooth circulation of particles towards the plasma and avoid turbulence that could create recirculation and back flow of powders above the hot zone of the chamber.
- these entrainment and cooling flows are chosen to minimize any non-uniformity in the thermal path in the outward radial direction away from axis 11 .
- the particles are processed volumetrically and uniformly and exit into an atmospheric fast quenching chamber below the exit nozzle of the plasma.
- the product upon solidification is collected in nylon or stainless steel filters, or quenched in distilled water in some applications, and analyzed for its microstructure and its mechanical, optical, and thermal properties.
- FIG. 7 the figure illustrates a procedure to produce densified and spheroidized particles using solution droplets.
- the desired chemical composition is first mixed according to the assigned proportions of reactants. Subsequently it is thoroughly stirred to yield a homogenous molecular mix of reactants.
- the solution is then poured into a stainless steel tank.
- a pressurized source of air is used to inject air into the tank and push the solution towards an injector nozzle similar to a nebulizer, and injected into the central feeding tube of the nebulizer where it emerges as a jet.
- another pressurized source is used to push air into an outer concentric tube of the nebulizer which penetrates the solution jet perpendicularly.
- these flows are chosen so as to allow a smooth circulation of droplets towards the plasma and avoid turbulence that could create recirculation and back flow of powders above the hot zone of the plasma chamber, as well as avoiding a disruption in the thermal path.
- FIG. 8 the figure illustrates a procedure to produce densified and spheroidized particles using uniform solution precursor droplets produced using a droplet maker.
- the desired solution's chemical composition is prepared by first mixing the assigned proportions of reactants. Subsequently, the solution is thoroughly stirred to yield a homogenous molecular mix of reactants. The solution is then pumped inside the reservoir of a droplet maker by means of a peristaltic pump, or a pressurized tank. Once the reservoir is full, a piezo transducer is activated which impinges an adequate perturbation onto the liquid solution in the reservoir.
- the solution emerges through a capillary nozzle as a continuous stream of uniform droplets exiting at a constant speed for a given drive frequency of the piezo.
- the nature of the droplets stream is monitored so that it is not in a burst mode or incidental mode but in the form of a jet with uniform droplets.
- This stream of droplets is then injected into the feeding tube of the dielectric plasma torch where it undergoes the same plasma process, and subsequently is transformed into a collection of dense and spheroidized particles as described in the paragraphs referring to FIG. 6 and FIG. 7 .
- this method has been applied to spheroidize particles 6 made of commercial Magnesia-Yttria (MgO—Y 2 O 3 ) solid powder particles obtained by the spray-drying technique from the INFRAMAT Corporation.
- the densified and spheroidized particles 6 exhibit a “pearl” like texture and morphology.
- this method has been applied to produce dense and spheroidized particles 6 directly from the injection of droplets of 7%-weight Yttria-Stabilized-Zirconia (7YSZ) solution precursor.
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US14/700,847 US9259785B2 (en) | 2012-11-13 | 2015-04-30 | Method for the densification and spheroidization of solid and solution precursor droplets of materials using microwave generated plasma processing |
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